KR20200020830A - Apparatus and method for continuous heat treatment of alloy workpieces or metal workpieces - Google Patents

Apparatus and method for continuous heat treatment of alloy workpieces or metal workpieces Download PDF

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KR20200020830A
KR20200020830A KR1020207001550A KR20207001550A KR20200020830A KR 20200020830 A KR20200020830 A KR 20200020830A KR 1020207001550 A KR1020207001550 A KR 1020207001550A KR 20207001550 A KR20207001550 A KR 20207001550A KR 20200020830 A KR20200020830 A KR 20200020830A
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South Korea
Prior art keywords
heat treatment
chamber
cooling
temperature
workpiece
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KR1020207001550A
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Korean (ko)
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KR102378901B1 (en
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칭장 왕
잉 뤄
지안펑 우
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푸젠 창팅 골든 드래곤 레어-어스 컴퍼니 리미티드
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Priority claimed from PCT/CN2018/109524 external-priority patent/WO2019148882A1/en
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    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/0006—Details, accessories not peculiar to any of the following furnaces
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/0062—Heat-treating apparatus with a cooling or quenching zone
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/56—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering characterised by the quenching agents
    • C21D1/613—Gases; Liquefied or solidified normally gaseous material
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/68—Temporary coatings or embedding materials applied before or during heat treatment
    • C21D1/72—Temporary coatings or embedding materials applied before or during heat treatment during chemical change of surfaces
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/773—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material under reduced pressure or vacuum
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D11/00—Process control or regulation for heat treatments
    • C21D11/005—Process control or regulation for heat treatments for cooling
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/0056—Furnaces through which the charge is moved in a horizontal straight path
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/0068—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for particular articles not mentioned below
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B5/00—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
    • F27B5/02—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated of multiple-chamber type
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B5/00—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
    • F27B5/04—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated adapted for treating the charge in vacuum or special atmosphere
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B5/00—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
    • F27B5/06—Details, accessories, or equipment peculiar to furnaces of these types
    • F27B5/18—Arrangement of controlling, monitoring, alarm or like devices
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B9/00—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity
    • F27B9/02—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity of multiple-track type; of multiple-chamber type; Combinations of furnaces
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B9/00—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity
    • F27B9/02—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity of multiple-track type; of multiple-chamber type; Combinations of furnaces
    • F27B9/028—Multi-chamber type furnaces
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D9/00—Cooling of furnaces or of charges therein
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/0536—Alloys characterised by their composition containing rare earth metals sintered
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67011—Apparatus for manufacture or treatment
    • H01L21/67098—Apparatus for thermal treatment
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67011—Apparatus for manufacture or treatment
    • H01L21/67155—Apparatus for manufacturing or treating in a plurality of work-stations
    • H01L21/67161—Apparatus for manufacturing or treating in a plurality of work-stations characterized by the layout of the process chambers
    • H01L21/67173—Apparatus for manufacturing or treating in a plurality of work-stations characterized by the layout of the process chambers in-line arrangement
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67011—Apparatus for manufacture or treatment
    • H01L21/67155—Apparatus for manufacturing or treating in a plurality of work-stations
    • H01L21/67184—Apparatus for manufacturing or treating in a plurality of work-stations characterized by the presence of more than one transfer chamber
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/677—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for conveying, e.g. between different workstations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/10—Inert gases
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2201/00—Treatment for obtaining particular effects
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2202/00—Physical properties
    • C22C2202/02—Magnetic
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B5/00—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
    • F27B5/06—Details, accessories, or equipment peculiar to furnaces of these types
    • F27B2005/062—Cooling elements
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D9/00—Cooling of furnaces or of charges therein
    • F27D2009/007—Cooling of charges therein
    • F27D2009/0072—Cooling of charges therein the cooling medium being a gas

Abstract

Nd-Fe-B계 소결 자성체 공작물의 연속 열처리 장치 및 방법은 순차적으로 연속 설치되는 제1 열처리 챔버, 제1 냉각 챔버, 제2 열처리 챔버, 제2 냉각 챔버, 및 상기 합금 공작물 또는 금속 공작물을 운반하기 위해 각 챔버 사이에 설치되는 이송 시스템을 포함하며, 제1 냉각 챔버와 제2 냉각 챔버는 모두 공랭 시스템을 채택하고, 제1 냉각 챔버의 냉각풍 온도는 25℃ 이상이면서, 상기 제1 열처리 챔버의 열처리 온도와 적어도 450℃의 차이가 있고, 상기 제2 냉각 챔버의 냉각풍 온도는 25℃ 이상이면서, 상기 제2 열처리 챔버의 열처리 온도와 적어도 300℃의 차이가 있다. 상기 연속 열처리 장치와 연속 열처리 방법은 냉각 속도와 생산 효율을 향상시킬 수 있으며, 제품의 성능과 일치성이 향상된다. Continuous heat treatment apparatus and method for Nd-Fe-B-based sintered magnetic workpiece conveys a first heat treatment chamber, a first cooling chamber, a second heat treatment chamber, a second cooling chamber, and the alloy workpiece or the metal workpiece sequentially installed in sequence. In order to include a transfer system installed between each chamber, the first cooling chamber and the second cooling chamber both adopt an air cooling system, the cooling air temperature of the first cooling chamber is 25 ℃ or more, while the first heat treatment chamber Is at least 450 ° C., and the cooling wind temperature of the second cooling chamber is 25 ° C. or more, and is at least 300 ° C. from the heat treatment temperature of the second heat treatment chamber. The continuous heat treatment apparatus and the continuous heat treatment method can improve the cooling rate and production efficiency, and improve the performance and consistency of the product.

Description

합금 공작물 또는 금속 공작물의 연속 열처리 장치 및 방법Apparatus and method for continuous heat treatment of alloy workpieces or metal workpieces

본 발명은 열처리 장치 및 열처리 방법에 관한 것으로서, 구체적으로는 합금 공작물 또는 금속 공작물의 연속 열처리 장치 및 연속 열처리 방법에 관한 것이다.The present invention relates to a heat treatment apparatus and a heat treatment method, and more particularly, to a continuous heat treatment apparatus and a continuous heat treatment method of an alloy workpiece or a metal workpiece.

네오디움 희토류 영구자석 재료는 현재 자기 에너지적(magnetic energy product)이 가장 높은 양산화된 자성체로서, 풍력발전, 서보모터, 가전용 압축기와 신에너지원 자동차의 모터 등 분야에 광범위하게 응용되고 있으며, 기타 자성체에 비해, 부피가 작고 효율이 높다는 등의 장점을 지닌다.Neodymium rare earth permanent magnet materials are currently the most mass-produced magnetic materials with the highest magnetic energy products, and are widely applied in the fields of wind power generation, servo motors, home compressors, and motors of new energy sources. Compared to the magnetic material, it has advantages such as small volume and high efficiency.

네오디움 재료는 통상적으로 제련, 파쇄, 압축, 소결, 열처리 등 공정을 거쳐야만 비로소 필요한 성능을 지닌 자성체를 획득할 수 있다. 그 중, 열처리는 제1단계 열처리 및 제2단계 열처리를 포함하며, 통상적으로 각각 800℃~950℃ 및 400℃~650℃이다.The neodymium material typically undergoes smelting, crushing, compression, sintering, heat treatment, etc. to obtain a magnetic material having required performance. Among them, the heat treatment includes a first stage heat treatment and a second stage heat treatment, and are usually 800 ° C to 950 ° C and 400 ° C to 650 ° C, respectively.

종래의 기술에서는 단일 챔버 열처리로를 이용하여 네오디움 재료에 대해 열처리를 실시하여, 승온과 강온이 반복하여 발생하고, 승온과 강온 속도를 제어하기 어려우며, 에너지 소모가 증가한다. 따라서, 종래의 단일 챔버 열처리로로는 성능과 일치성이 양호한 고성능 네오디움 재료를 제작하기가 어렵다. 또한, 단일 챔버 열처리로는 일반적으로 원기둥형 노체(furnace body)이고, 열원은 원기둥형 노체의 내벽이며, 재료가 대부분 다중 열의 입체적인 적층 방식으로 배치되기 때문에, 상이한 위치의 재료들로부터 열원 사이의 거리가 각기 달라지게 된다. 따라서 노내 온도의 일치성과 균일성이 떨어지며, 특히 코어부의 재료와 바깥 둘레의 재료에서 온도차가 나타난다. 이러한 배치 방식 또한 단일 챔버 열처리로의 신속한 온도 하강 능력을 제한한다.In the prior art, a single chamber heat treatment furnace is used to heat-treat the neodymium material, so that temperature and temperature are repeatedly generated, it is difficult to control the temperature and temperature rate, and energy consumption is increased. Therefore, it is difficult to fabricate high performance neodymium materials with good performance and consistency with conventional single chamber heat treatment furnaces. In addition, the single chamber heat treatment furnace is generally a cylindrical furnace body, the heat source is the inner wall of the cylindrical furnace body, and the distance between the heat sources from the materials at different positions, since the material is mostly arranged in a multi-row three-dimensional stacking manner. Will be different. Therefore, the uniformity and uniformity of the temperature in the furnace is inferior, and the temperature difference appears in the material of the core part and the material of the outer circumference. This arrangement also limits the ability to quickly drop temperatures into a single chamber heat treatment furnace.

상기 문제를 감안하여, 본 발명은 냉각 속도와 생산 효율을 높여 제품의 일관성을 향상시킬 수 있는 합금 공작물 또는 금속 공작물의 연속 열처리 장치를 제공한다.In view of the above problems, the present invention provides a continuous heat treatment apparatus of an alloy workpiece or a metal workpiece that can improve the cooling rate and production efficiency to improve product consistency.

본 발명이 채택한 기술방안은 다음과 같다:The technical solutions adopted by the present invention are as follows:

합금 공작물 또는 금속 공작물의 연속 열처리 장치에 있어서, 기밀장치를 통해 순차적으로 설치되는 제1 열처리 챔버, 제1 냉각 챔버, 제2 열처리 챔버, 제2 냉각 챔버, 및 상기 합금 공작물 또는 금속 공작물을 이송하기 위해 각 챔버 사이에 설치되는 이송 시스템을 포함하고, 상기 제1 냉각 챔버와 상기 제2 냉각 챔버는 모두 공랭 시스템을 채택하며, 상기 제1 냉각 챔버의 냉각풍 온도는 25℃ 이상이면서, 상기 제1 열처리 챔버의 열처리 온도와 적어도 450℃의 차이가 있고, 상기 제2 냉각 챔버의 냉각풍 온도는 25℃ 이상이면서, 상기 제2 열처리 챔버의 열처리 온도와 적어도 300℃의 차이가 있으며, 상기 냉각 챔버의 압력은 50kPa-100kPa인 것을 특징으로 한다.A continuous heat treatment apparatus for an alloy workpiece or a metal workpiece, the method comprising: conveying a first heat treatment chamber, a first cooling chamber, a second heat treatment chamber, a second cooling chamber, and the alloy workpiece or the metal workpiece sequentially installed through an airtight device. And a transfer system installed between each chamber, wherein both the first cooling chamber and the second cooling chamber adopt an air cooling system, and the cooling air temperature of the first cooling chamber is 25 ° C. or higher, There is a difference between the heat treatment temperature of the heat treatment chamber and at least 450 ° C., the cooling wind temperature of the second cooling chamber is 25 ° C. or more, and a difference between the heat treatment temperature of the second heat treatment chamber and at least 300 ° C., and The pressure is characterized in that 50kPa-100kPa.

본 발명은 열처리 챔버와 냉각 챔버(공랭 시스템 방식 사용)를 단독으로 설치하고, 냉각 챔버의 냉각풍 온도를 한정하는 방식을 채택하여, 재료의 열처리가 완료된 후, 필요한 냉각 공정에 따라, 열처리 후 고온 구간의 신속하고 균일한 냉각을 구현함으로써, 합금 공작물 또는 금속 공작물의 입계 미세조직의 위상 성분과 분포를 최적화할 수 있다. 공랭 시스템은 강제 대류 열교환이 가능하여, 재료의 열에너지를 신속하게 배출시키며, 송풍기의 변속을 통해, 냉각 속도의 제어를 구현할 수 있다.According to the present invention, after a heat treatment chamber and a cooling chamber (using an air cooling system method) are installed alone, a method of limiting the cooling wind temperature of the cooling chamber is adopted, and the heat treatment of the material is completed, according to the required cooling process, By realizing rapid and uniform cooling of the sections, it is possible to optimize the phase component and distribution of the grain boundary microstructure of the alloy workpiece or the metal workpiece. The air-cooled system is capable of forced convection heat exchange, quickly discharging the thermal energy of the material, and by controlling the speed of the blower, it is possible to realize the control of the cooling rate.

본 발명에서, 냉각 챔버의 압력이 50kPa-100kPa인 설정은 본 업계의 통상적인 선택이며, 따라서, 실시예에서는 상기 함량 범위에 대한 시험과 검증을 생략하였다.In the present invention, a setting in which the pressure of the cooling chamber is 50 kPa-100 kPa is a common choice in the art, and therefore, the examples omit testing and verification of the content range.

본 발명의 다른 목적은 냉각 속도와 생산 효율을 높여 제품의 성능과 일치성을 향상시킬 수 있는 합금 공작물 또는 금속 공작물의 연속 열처리 방법을 제공하고자 하는데 있다. Another object of the present invention is to provide a continuous heat treatment method of an alloy workpiece or a metal workpiece that can increase the cooling rate and production efficiency to improve product performance and consistency.

본 발명이 채택한 기술방안은 다음과 같다:The technical solutions adopted by the present invention are as follows:

합금 공작물 또는 금속 공작물의 연속 열처리 방법에 있어서, 상호 기밀되는 분리 챔버에서 순차적으로 실시되는 제1단계 열처리, 제1단계 공냉각 처리, 제2단계 열처리, 및 제2단계 공냉각 처리를 포함하며, 상기 제1단계 공냉각 처리의 냉각풍 온도는 25℃ 이상이면서, 상기 제1단계 열처리의 열처리 온도와 적어도 450℃의 차이가 있고, 상기 제2단계 공냉각 처리의 냉각풍 온도는 25℃ 이상이면서, 상기 제2단계 열처리의 열처리 온도와 적어도 300℃의 차이가 있는 것을 특징으로 한다. A continuous heat treatment method for an alloy workpiece or a metal workpiece, the method comprising: a first stage heat treatment, a first stage air cooling treatment, a second stage heat treatment, and a second stage air cooling treatment, which are sequentially performed in a mutually hermetic separation chamber, While the cooling wind temperature of the first stage air cooling treatment is 25 ° C. or more, there is a difference of at least 450 ° C. from the heat treatment temperature of the first stage heat treatment, and the cooling wind temperature of the second stage air cooling treatment is 25 ° C. or more. In addition, there is a difference between the heat treatment temperature of the second step heat treatment at least 300 ℃.

설명해두어야 할 점으로, 본 발명에 공개된 숫자 범위는 이러한 범위 내의 모든 점값(point value)을 포함한다.It should be noted that the numerical range disclosed in the present invention includes all point values within this range.

이하 실시예를 결합하여 본 발명에 대해 좀 더 상세히 설명한다.The present invention will be described in more detail with reference to the following examples.

바람직한 실시방식에서, 상기 합금 공작물은 Nd-Fe-B계 소결 자성체이다. 그 이유는, 출원인이 연구하는 과정에서, Nd-Fe-B계 소결 자성체가 분리 챔버에서 열처리 및 고온 구간에서의 신속한 냉각을 거친 후, 제품의 직각도(squareness), 고유 보자력(intrinsic coercive force)과 제품의 일치성이 향상될 수 있으며, 특히 고유 보자력이 현저히 향상될 수 있음을 발견하였기 때문이다. 이러한 작용 메커니즘은 현 단계에서는 아직까지는 불명확하다. In a preferred embodiment, the alloy workpiece is an Nd-Fe-B based sintered magnetic body. The reason is that, in the course of the applicant's research, after the Nd-Fe-B-based sintered magnetic material undergoes heat treatment and rapid cooling in a high temperature section in the separation chamber, the squareness and intrinsic coercive force of the product This is because the concordance between the product and the product can be improved, and in particular, the intrinsic coercivity can be significantly improved. This mechanism of action is still unclear at this stage.

바람직한 실시방식에서, 상기 공랭 시스템은 불활성 가스를 채택한 공랭 시스템이다. 여기서의 불활성 가스는 헬륨, 네온, 아르곤, 크립톤, 제논, 라돈 또는 질소가스 등 상기 입계 확산 처리, 냉각 처리와 열처리 과정에서 합금 공작물 또는 금속 공작물과 반응하지 않는 가스 중에서 선택된다.In a preferred embodiment, the air cooling system is an air cooling system employing an inert gas. The inert gas here is selected from a gas which does not react with an alloy workpiece or a metal workpiece in the grain boundary diffusion treatment, cooling treatment and heat treatment process such as helium, neon, argon, krypton, xenon, radon or nitrogen gas.

바람직한 실시방식에서, 상기 제1 열처리 챔버의 열처리 온도는 800℃~950℃이고, 상기 제1 냉각 챔버의 냉각풍 온도는 25℃~150℃이며, 상기 제2 열처리 챔버의 열처리 온도는 400℃~650℃이고, 상기 제2 냉각 챔버의 냉각풍 온도는 25℃~100℃이다. 이와 같이 하면 네오디움 재료가 신속하게 공융점(eutectic point)을 통과할 수 있어, 양호한 직각도와 보자력을 획득할 수 있다.In a preferred embodiment, the heat treatment temperature of the first heat treatment chamber is 800 ℃ ~ 950 ℃, the cooling wind temperature of the first cooling chamber is 25 ℃ ~ 150 ℃, the heat treatment temperature of the second heat treatment chamber is 400 ℃ ~ It is 650 degreeC, and the cooling wind temperature of the said 2nd cooling chamber is 25 degreeC-100 degreeC. This allows the neodymium material to quickly pass through the eutectic point, thereby obtaining good squareness and coercive force.

그 중, 제1 열처리 챔버의 온도 800℃~950℃와 제2 열처리 챔버의 열처리 온도 400℃~650℃ 등의 함량 범위는 Nd-Fe-B계 소결 자성체 분야에서 열처리 공정의 통상적인 선택이며, 따라서, 실시예에서는 상기 함량 범위에 대해 시험과 검증을 생략하였다.Among them, the content range of the temperature of 800 ° C to 950 ° C of the first heat treatment chamber and the heat treatment temperature of 400 ° C to 650 ° C of the second heat treatment chamber is a typical selection of the heat treatment process in the field of Nd-Fe-B-based sintered magnetic body, Therefore, in the examples, the test and verification for the content range was omitted.

일반적으로, 제1 냉각 챔버, 제2 냉각 챔버의 초기 온도는 상응하는 냉각풍 온도와 동일하다.In general, the initial temperature of the first cooling chamber and the second cooling chamber is equal to the corresponding cooling wind temperature.

바람직한 실시방식에서, 상기 제1 열처리 챔버는 사각형 구조이면서, 상기 사각형 구조 내벽에 서로 반대 방향으로 설치되는 2개의 가열 영역을 포함하고, 상기 합금 공작물 또는 상기 금속 공작물은 상기 사각형 구조 중앙부의 재료 홀더에 직접 배치되거나, 또는 상기 합금 공작물 또는 상기 금속 공작물은 먼저 재료 박스 내에 담긴 후 상기 재료 박스가 상기 사각형 구조 중앙의 재료 홀더에 배치되며; 마찬가지로, 상기 제2 열처리 챔버는 사각형 구조이면서, 상기 사각형 구조 내벽에 서로 반대 방향으로 설치되는 2개의 가열 영역을 포함하고, 상기 합금 공작물 또는 상기 금속 공작물은 상기 사각형 구조 중앙부의 재료 홀더에 직접 배치되거나, 또는 상기 합금 공작물 또는 상기 금속 공작물은 먼저 재료 박스 내에 담긴 후 상기 재료 박스가 상기 사각형 구조 중앙의 재료 홀더에 배치된다. 상기 구조를 통해 재료 온도의 높은 균일성을 구현하고, 온도 파동을 제어할 수 있다.In a preferred embodiment, the first heat treatment chamber has a rectangular structure and includes two heating zones installed in opposite directions on the inner wall of the rectangular structure, wherein the alloy workpiece or the metal workpiece is placed in a material holder in the center of the rectangular structure. Or the alloy workpiece or the metal workpiece is first contained in a material box and then the material box is placed in a material holder in the center of the rectangular structure; Similarly, the second heat treatment chamber has a rectangular structure and includes two heating zones installed in opposite directions on the inner wall of the rectangular structure, and the alloy workpiece or the metal workpiece is disposed directly in a material holder in the center of the rectangular structure. Or the alloy workpiece or the metal workpiece is first contained in a material box and then the material box is placed in a material holder in the center of the rectangular structure. The structure enables high uniformity of material temperature and control of temperature fluctuations.

바람직한 실시방식에서, 상기 가열 영역의 면적은 상기 재료 홀더의 종단면 면적을 초과한다. 이와 같이 하면, 모든 재료 박스가 균일하게 열처리를 받도록 보장할 수 있어, 열처리 후의 합금 공작물 또는 금속 공작물의 성능을 일치시킬 수 있다.In a preferred embodiment, the area of the heating zone exceeds the longitudinal cross-sectional area of the material holder. In this way, it is possible to ensure that all the material boxes are uniformly heat treated, so that the performance of the alloy work or the metal work after heat treatment can be matched.

바람직한 실시방식에서, 상기 제2 열처리 챔버 중, 상기 재료 박스 또는 합금 공작물 또는 금속 공작물로부터 서로 반대 방향으로 설치되는 2개의 상기 가열 영역의 거리는 동일하여, 2cm-30cm이며, 바람직하게는 5cm-20cm이다. 출원인은 생산 과정에서, Nd-Fe-B계 자성체는 2단계 템퍼링 온도차에 대단히 민감하여, 2단계 템퍼링 온도차를 제어하면 Nd-Fe-B계 자성체 성능과 각 영역의 Nd-F-B계 자성체의 일치성을 현저히 향상시킬 수 있음을 발견하였다. 본 출원에서, 재료 박스를 가열 영역에 가깝게 설치하는 방식을 선택하여, 특히 거리를 5cm-20cm로 제어한 후, 최적의 실시방식에서, 각 영역의 재료 박스 또는 각 영역의 합금 공작물 또는 각 영역의 금속 공작물 또는 재료 박스의 상이한 영역의 온도차를 ±5℃ 이내로 제어할 수 있었으며, 재료 온도의 높은 균일성을 구현하여 동일 회분(batch)의 Nd-Fe-B계 자성체의 성능의 일치성이 대단히 높아졌다.In a preferred embodiment, the distance of the two heating zones which are installed in the opposite direction from the material box or the alloy workpiece or the metal workpiece in the second heat treatment chamber is the same, preferably 2 cm-30 cm, preferably 5 cm-20 cm. . In the production process, Applicants note that the Nd-Fe-B-based magnetic material is very sensitive to the two-step tempering temperature difference. It has been found that can be significantly improved. In the present application, the method of installing the material box close to the heating zone is selected, in particular, the distance is controlled from 5 cm to 20 cm, and in an optimum embodiment, the material box of each zone or the alloy workpiece of each zone or the The temperature difference of different regions of the metal workpiece or the material box can be controlled within ± 5 ° C, and the high uniformity of the material temperature is realized, and the performance of the same batch of Nd-Fe-B-based magnetic materials is greatly increased. .

바람직한 실시방식에서, 상기 Nd-Fe-B계 자성체는 TRE(희토류 총 함량)가 28.8wt%-34.0wt%인 Nd-Fe-B계 자성체이며, 바람직하게는 TRE(희토류 총 함량)가 28.8wt%-30.5wt%인 Nd-Fe-B계 자성체이다. 연구 과정에서, TRE(희토류 총 함량)가 28.8wt%-30.5wt%인 자성체는 2단계 템퍼링 온도차에 가장 민감하며, 열처리 온도 제어에 대한 요구가 더욱 높다는 점을 발견하였다.In a preferred embodiment, the Nd-Fe-B-based magnetic material is Nd-Fe-B-based magnetic material having a TRE (total rare earth content) of 28.8wt% -34.0wt%, preferably TRE (total rare earth content) is 28.8wt It is an Nd-Fe-B based magnetic material of% -30.5wt%. In the course of the study, it was found that magnetic materials with a total rare earth content (TRE) of 28.8wt% -30.5wt% were most sensitive to the two-stage tempering temperature difference and the demand for heat treatment temperature control was higher.

본 발명에서 언급한 Nd-Fe-B계 자성체는 Nd2Fe14B형 주상(main phase)을 포함하는 자석이다.The Nd-Fe-B-based magnetic material mentioned in the present invention is a magnet including a Nd 2 Fe 14 B type main phase.

바람직한 실시방식에서, 기밀장치를 통해 순차적으로 설치되는 제1 승온 챔버, 제2 승온 챔버, 제1 열처리 챔버, 제1 냉각 챔버, 제3 승온 챔버, 제2 열처리 챔버 및 제2 냉각 챔버를 포함한다. 이는 800℃~950℃까지 승온시키는 시간이 대략 제1 열처리 챔버의 열처리 시간의 2배 정도이기 때문이며, 2개의 승온 챔버의 설치를 통해, 2개의 승온 챔버의 처리 시간이 입계 확산 챔버의 열처리 시간과 같아지도록 속도를 일치시킴으로써, 생산이 질서 있게 진행될 수 있다.In a preferred embodiment, the method includes a first temperature raising chamber, a second temperature raising chamber, a first heat treatment chamber, a first cooling chamber, a third temperature raising chamber, a second heat treatment chamber and a second cooling chamber sequentially installed through an airtight device. . This is because the time for raising the temperature to 800 ° C. to 950 ° C. is approximately twice the heat treatment time of the first heat treatment chamber, and through the installation of the two temperature raising chambers, the processing time of the two temperature raising chambers is the same as the heat treatment time of the grain boundary diffusion chamber. By matching the speeds to be equal, production can proceed in order.

바람직한 실시방식에서, 상기 제2단계 열처리 중, 상이한 영역의 상기 합금 공작물 또는 금속 공작물의 온도차는 ±5℃ 이하이다.In a preferred embodiment, during the second stage heat treatment, the temperature difference of the alloy workpiece or the metal workpiece in different regions is ± 5 ° C. or less.

바람직한 실시방식에서, 상기 제1단계 냉각 처리 중, 상기 합금 공작물 또는 상기 금속 공작물의 최초 10min의 평균 냉각 속도는 6℃/min-15℃/min이고, 상기 제2단계 냉각 처리 중, 상기 합금 공작물 또는 금속 공작물의 최초 10min의 평균 냉각 속도는 6℃/min-15℃/min이다.In a preferred embodiment, the average cooling rate of the first 10 min of the alloy workpiece or the metal workpiece during the first stage cooling treatment is 6 ° C./min-15° C./min, and the alloy workpiece during the second stage cooling treatment. Or the average cooling rate of the first 10 min of the metal workpiece is 6 ° C./min-15° C./min.

본 발명에서는 부단한 시험 검증을 통해, 최초 10min의 평균 냉각 속도를 선택하여 모니터링하였으며, 물론, 제품의 필요에 따라, 최초 5min-30min의 평균 냉각 속도를 선택하여 모니터링할 수도 있다.In the present invention, through constant test verification, the average cooling rate of the first 10min was selected and monitored, and, of course, the average cooling rate of the first 5min-30min may be selected and monitored according to the needs of the product.

각 실시예에서 획득된 소결 자석은 모두 이하 검출 방식을 이용하여 측정하였다.The sintered magnets obtained in each example were all measured using the following detection method.

자기 성능 평가 과정: 소결 자석은 중국 계량원의 NIM-10000H형 BH 벌크 희토류 영구자석 비파괴 측정 시스템으로 자기 성능 검출을 실시하였다. Magnetic performance evaluation process: The sintered magnet was subjected to magnetic performance detection by NIM-10000H type BH bulk rare earth permanent magnet nondestructive measurement system of China Metrology.

실시예Example 1 One

연속 열처리 장치는 순차적으로 연속 설치되는 제1 승온 챔버, 제2 승온 챔버, 제1 열처리 챔버, 제1 냉각 챔버, 제3 승온 챔버, 제2 열처리 챔버와 제2 냉각 챔버를 포함하며, 제1 승온 챔버, 제2 승온 챔버, 제1 열처리 챔버, 제1 냉각 챔버, 제3 승온 챔버, 제2 열처리 챔버와 제2 냉각 챔버 사이에 기밀 밸브, 및 각 챔버 사이에 설치되어 Nd-Fe-B계 소결 자성체를 운반하기 위한 이송 시스템이 설치된다.The continuous heat treatment apparatus includes a first temperature raising chamber, a second temperature raising chamber, a first heat treatment chamber, a first cooling chamber, a third temperature raising chamber, a second heat treatment chamber, and a second cooling chamber which are sequentially installed in succession. Chamber, second heating chamber, first heat treatment chamber, first cooling chamber, third heating chamber, a gas tight valve between the second heat treatment chamber and the second cooling chamber, and is installed between each chamber and sintered Nd-Fe-B-based A transport system for transporting the magnetic material is installed.

연속 열처리 과정은 다음과 같다:The continuous heat treatment process is as follows:

(1) 재료 장입(1) charging materials

질량백분율(wt%)에 따라, 조성이 Pr 7.25%, Nd 21.75%, Dy 1.5%, Fe bal., B 0.97%, Cu 0.15%, Ga 0.2%, Nb 0.2%, Co 0.8%인 원료를 취하여, 제련, 스트립 캐스팅(strip casting), 수소파쇄, 기류파쇄, 압형 및 소결을 통해 Nd-Fe-B계 소결 자성체를 획득한다.According to the mass percentage (wt%), raw materials having a composition of Pr 7.25%, Nd 21.75%, Dy 1.5%, Fe bal., B 0.97%, Cu 0.15%, Ga 0.2%, Nb 0.2%, Co 0.8% Nd-Fe-B-based sintered magnetic bodies are obtained through smelting, strip casting, hydrogen crushing, airflow crushing, pressing and sintering.

검출을 거친 Nd-Fe-B계 소결 자성체의 성능은 Hcj=16.50kOe, Br=13.70kGs이고, 직각도는 98%이다.The performance of the detected Nd-Fe-B-based sintered magnetic body was Hcj = 16.50 kOe, Br = 13.70 kGs, and the squareness was 98%.

Nd-Fe-B계 소결 자성체를 관통공을 구비한 재료 박스 내에 담고, 재료 박스를 2열로 적층한 후, 재료 홀더에 배치하여 제1 승온 챔버 내로 이송한다. 특히 상이한 생산 요구에 따라, 변환된 실시예에서는 밀폐식 재료 박스를 사용할 수도 있음을 언급해둔다. The Nd-Fe-B-based sintered magnetic body is contained in a material box having a through hole, the material boxes are stacked in two rows, and then placed in a material holder and transferred into the first temperature raising chamber. It is noted that, depending on the different production requirements, in the converted embodiment, it is also possible to use a sealed material box.

(2) 제1단계 승온(2) The first stage temperature rise

제1 승온 챔버의 진공도가 100Pa에 도달하였을 때 가열 프로세스를 작동시켜, 실온으로부터 시작하여 165min 동안 승온시키고, 온도가 370℃-400℃에 도달한 후, 15min 동안 보온한다. 보온 종료 후, 재료 박스가 장착된 재료 홀더를 제1 승온 챔버로부터 제2 승온 챔버로 이송한다.The heating process is started when the vacuum degree of the first heating chamber reaches 100 Pa, starting from room temperature for 165 min, warming for 15 min after the temperature reaches 370 ° C.-400 ° C. After the end of heat retention, the material holder with the material box is transferred from the first temperature raising chamber to the second temperature raising chamber.

(3) 제2단계 승온(3) The second stage temperature rise

재료 박스가 장착된 재료 홀더가 제2 승온 챔버로 진입한 후, 진공도가 100Pa에 도달하였을 때, 165min 동안 가열하여 승온시키고, 온도가 800℃-850℃에 도달한 후, 15min 동안 보온한다. 보온 종료 후, 재료 박스가 장착된 재료 홀더를 제2 승온 챔버로부터 제1 열처리 챔버로 이송한다.After the material holder equipped with the material box enters the second temperature raising chamber, when the degree of vacuum reaches 100 Pa, it is heated by heating for 165 min, and is heated for 15 min after the temperature reaches 800 ° C.-850 ° C. After the end of heat retention, the material holder with the material box is transferred from the second temperature raising chamber to the first heat treatment chamber.

(4) 제1단계 열처리(4) First stage heat treatment

제1 열처리 챔버는 사각형 구조이면서, 사각형 구조 내벽에 서로 반대 방향으로 설치되는 2개의 가열 영역을 포함하며, 가열 영역의 면적은 재료 홀더의 종단면 면적을 초과한다. 재료 박스는 제1 열처리 챔버로 진입한 후, 2개의 가열 영역과 모두 25cm의 거리인 위치에 배치된다.The first heat treatment chamber has a rectangular structure and includes two heating regions installed in opposite directions on the inner wall of the rectangular structure, the area of the heating region exceeding the longitudinal cross-sectional area of the material holder. After entering the first heat treatment chamber, the material box is placed at a location that is both 25 cm away from the two heating zones.

진공도가 100Pa에 도달하였을 때, 10min 동안 가열하여 승온시키고, 제1 열처리 챔버의 열처리 온도(상이한 재료 박스 내의 각기 다른 위치에서 검출한다)가 880℃-895℃에 이르면 170min 동안 보온한다. 보온 종료 후, 재료 박스가 장착된 재료 홀더를 제1 열처리 챔버로부터 제1 냉각 챔버로 이송한다.When the degree of vacuum reaches 100 Pa, it is heated for 10 min to raise the temperature, and when the heat treatment temperature (detected at different positions in different material boxes) of the first heat treatment chamber reaches 880 ° C-895 ° C, it is kept warm for 170min. After the end of the warming, the material holder equipped with the material box is transferred from the first heat treatment chamber to the first cooling chamber.

(5) 제1단계 냉각(5) first stage cooling

재료 박스가 장착된 재료 홀더가 제1 냉각 챔버로 진입한 후, 진공시키고 냉각 챔버로 78kPa인 불활성 가스를 주입한 다음, 송풍기로 순환 냉각을 실시하며, 냉각 시간은 180min이다. 제1 냉각 챔버의 불활성 가스 온도는 표 1을 참조한다. 불활성 가스 온도는 흡기식 순환풍의 공기배출구 부위에서 검출한다.After the material holder equipped with the material box enters the first cooling chamber, it is evacuated and injected with 78 kPa of inert gas into the cooling chamber, followed by circulating cooling with a blower, and the cooling time is 180 min. See Table 1 for the inert gas temperature of the first cooling chamber. The inert gas temperature is detected at the air outlet portion of the intake circulation wind.

(6) 제3단계 승온(6) Third stage temperature rise

2열로 적층된 재료 박스가 제3 승온 챔버로 진입한 후, 진공도가 100Pa에 도달하였을 때, 165min 동안 가열하여 승온시키고, 온도가 460℃-470℃에 이르면 15min 동안 보온한다. 보온 종료 후, 재료 박스가 장착된 재료 홀더를 제3 승온 챔버로부터 제2 열처리 챔버로 이송한다.After two rows of stacked material boxes enter the third temperature raising chamber, when the vacuum degree reaches 100 Pa, the temperature is increased by heating for 165 min, and the temperature is kept at 460 ° C.-470 ° C. for 15 min. After the end of heat retention, the material holder with the material box is transferred from the third temperature raising chamber to the second heat treatment chamber.

(7) 제2단계 열처리(7) second stage heat treatment

제2 열처리 챔버는 사각형 구조이면서, 사각형 구조 내벽에 서로 반대 방향으로 설치되는 2개의 가열 영역을 포함하며, 가열 영역의 면적은 재료 홀더의 종단면 면적을 초과한다. 재료 박스는 제2 열처리 챔버로 진입한 후, 2개의 가열 영역과 모두 25cm의 거리인 위치에 배치된다.The second heat treatment chamber has a rectangular structure and includes two heating regions installed in opposite directions on the inner wall of the rectangular structure, the area of the heating region exceeding the longitudinal cross-sectional area of the material holder. After entering the second heat treatment chamber, the material box is placed at a location that is both 25 cm away from the two heating zones.

진공도가 100Pa에 도달하였을 때, 15min 동안 가열하여 승온시키고, 열처리 온도(상이한 재료 박스 내의 각기 다른 위치에서 검출한다)가 500℃-515℃에 이른 후, 165min 동안 보온한다. 보온 종료 후, 재료 박스가 장착된 재료 홀더를 제2 열처리 챔버로부터 제2 냉각 챔버로 이송한다.When the degree of vacuum reaches 100 Pa, it is heated for 15 min to raise the temperature, and after the heat treatment temperature (detected at different positions in different material boxes) reaches 500 ° C-515 ° C, it is kept warm for 165min. After the end of heat retention, the material holder equipped with the material box is transferred from the second heat treatment chamber to the second cooling chamber.

(8) 제2단계 냉각(8) second stage cooling

재료 박스가 장착된 재료 홀더가 제2 냉각 챔버로 진입한 후, 진공시키고, 냉각 챔버로 78kPa인 불활성 가스를 주입한 다음, 송풍기로 순환 냉각을 실시하며, 냉각 시간은 180min이다. 재료 박스가 장착된 재료 홀더를 로(furnace)에서 인출한다. 제2 냉각 챔버의 불활성 가스 온도는 표 1을 참조하며, 불활성 가스 온도는 흡기식 순환풍의 공기배출구 부위에서 검출한다.After the material holder equipped with the material box enters the second cooling chamber, it is evacuated, an inert gas of 78 kPa is injected into the cooling chamber, and circulating cooling is performed with a blower, and the cooling time is 180 min. The material holder with the material box is withdrawn from the furnace. The inert gas temperature of the 2nd cooling chamber refers to Table 1, and an inert gas temperature is detected in the air outlet part of the intake type circulation wind.

이와 같이, 재료 박스가 장착된 재료 홀더는 제1 승온 챔버에서 승온과 단시간의 보온이 실시된 후, 제2 승온 챔버로 진입하여 승온 및 단시간의 보온이 실시된다. 제1 열처리 챔버의 보온이 종료된 후, 제1 냉각 챔버로 진입하여 냉각되고, 제1 냉각 챔버의 냉각이 종료된 후, 제3 승온 챔버로 진입하여 승온과 단시간의 보온이 실시된다. 제3 승온 챔버의 보온이 종료된 후, 제2 열처리 챔버로 진입하여 단시간의 승온과 보온이 실시되고, 보온 종료 후, 제2 냉각 챔버로 진입하여 냉각이 실시되며, 냉각 종료 후 인출된다.As described above, the material holder on which the material box is mounted is heated in the first temperature raising chamber and kept warm for a short time. Then, the material holder enters the second temperature rising chamber to perform the temperature rising and the warming for a short time. After the heat retention of the first heat treatment chamber is completed, the heat is entered into the first cooling chamber and cooled, and after the cooling of the first cooling chamber is completed, the heat treatment is performed in the third temperature raising chamber to increase the temperature and maintain the heat for a short time. After the heat retention of the third temperature increase chamber is completed, the second heat treatment chamber enters the second heat treatment chamber, and the temperature rises and heat retains for a short time. After the completion of the heat retention, the heat enters the second cooling chamber, the cooling is performed, and the cooling is terminated.

상기 열처리와 냉각 처리를 거친 후의 자석 성능은 표 1과 같다.The magnet performance after the heat treatment and cooling treatment is shown in Table 1.

표 1: 제1, 제2 냉각 챔버의 불활성 가스 온도, 및 열처리와 냉각 처리를 거친 후의 자석 성능Table 1: Inert gas temperatures in the first and second cooling chambers, and magnet performance after heat treatment and cooling
항목
Item 제1 냉각 챔버의 불활성 가스 온도(℃)Inert gas temperature (° C.) of the first cooling chamber 제2 냉각 챔버의 불활성 가스 온도(℃)Inert gas temperature (° C.) of the second cooling chamber
열처리와 냉각 처리 후
After heat treatment and cooling treatment Br(kGs)Br (kGs) Hcj(KOe)Hcj (KOe) SQ(%)SQ (%) 비교예 1.1Comparative Example 1.1 460-470460-470 370-380370-380 13.6913.69 18.618.6 9696 비교예 1.2Comparative Example 1.2 430-440430-440 70-8070-80 13.7013.70 18.818.8 9797 비교예 1.3Comparative Example 1.3 250-260250-260 350-360350-360 13.6813.68 18.718.7 9797 실시예 1.1Example 1.1 420-430420-430 190-200190-200 13.7113.71 19.319.3 9898 실시예 1.2Example 1.2 320-330320-330 150-160150-160 13.6913.69 19.419.4 9898 실시예 1.3Example 1.3 310-320310-320 70-8070-80 13.7013.70 19.719.7 9999 실시예 1.4Example 1.4 90-10090-100 90-10090-100 13.7013.70 19.619.6 9898 실시예 1.5Example 1.5 25-3525-35 25-3525-35 13.7213.72 19.819.8 9999 실시예 1.6Example 1.6 200-210200-210 25-3525-35 13.7013.70 19.719.7 9999 비교예 1.4Comparative Example 1.4 10-2010-20 10-2010-20 소량의 자석 표면에 균열이 나타났다Cracks appeared on a small amount of magnet surface

검출 결과, 실시예 1.4, 실시예 1.5와 실시예 1.6의 제1단계 냉각 처리 과정에서, Nd-Fe-B계 소결 자성체의 최초 10min의 평균 냉각 속도는 6℃/min-15℃/min이고, 실시예 1.3, 실시예 1.4, 실시예1.5와 실시예1.6의 제2단계 냉각 처리 과정에서, Nd-Fe-B계 소결 자성체의 최초 10min의 평균 냉각 속도는 6℃/min-15℃/min이었다. 그러나 실시예 1.1, 실시예1.2와 실시예 1.3의 제1단계 냉각 처리 과정에서, Nd-Fe-B계 소결 자성체의 최초 10min의 평균 냉각 속도는 6℃/min 미만이었고, 실시예 1.1과 실시예 1.2의 제2단계 냉각 처리 과정에서, Nd-Fe-B계 소결 자성체의 최초 10min의 평균 냉각 속도 역시 마찬가지로 6℃/min 미만이었다.As a result of the detection, in the first stage cooling process of Example 1.4, Example 1.5 and Example 1.6, the average cooling rate of the first 10 minutes of the Nd-Fe-B-based sintered magnetic body is 6 ° C / min-15 ° C / min, In the second stage cooling treatment process of Example 1.3, Example 1.4, Example 1.5 and Example 1.6, the average cooling rate of the first 10 minutes of the Nd-Fe-B-based sintered magnetic body was 6 ° C / min-15 ° C / min . However, in the first stage cooling process of Example 1.1, Example 1.2 and Example 1.3, the average cooling rate of the first 10 min of the Nd-Fe-B-based sintered magnetic body was less than 6 ℃ / min, Example 1.1 and Example In the second stage cooling treatment of 1.2, the average cooling rate of the first 10 min of the Nd-Fe-B-based sintered magnetic body was also less than 6 ° C / min.

표 1에서 볼 수 있듯이, 제1 냉각 챔버의 냉각풍 온도가 25℃ 이상이고, 제1 열처리 챔버의 열처리 온도보다 적어도 450℃ 낮으며, 이와 동시에 제2 냉각 챔버의 불활성 가스 온도가 25℃ 이상이고, 제2 열처리 챔버의 열처리 온도보다 적어도 300℃ 낮을 때, 열처리 후의 자성체의 자기 성능이 더욱 우수하며, 특히 Hcj가 뚜렷하게 향상되고, SQ가 개선되었다. 이는 상기 온도 구간 내에서 자성체의 열처리 후 고온 구간의 냉각 속도가 향상되어, 입계 미세 조직의 위상 성분과 분포를 최적화하는데 도움이 되기 때문이다.As can be seen from Table 1, the cooling wind temperature of the first cooling chamber is at least 25 ℃, at least 450 ℃ lower than the heat treatment temperature of the first heat treatment chamber, and at the same time the inert gas temperature of the second cooling chamber is at least 25 ℃ When the temperature is at least 300 ° C lower than the heat treatment temperature of the second heat treatment chamber, the magnetic performance of the magnetic body after heat treatment is more excellent, in particular, the Hcj is markedly improved and the SQ is improved. This is because the cooling rate of the high temperature section after the heat treatment of the magnetic material within the temperature section is improved, which helps to optimize the phase component and distribution of the grain boundary microstructure.

실시예Example 2 2

연속 열처리 장치는 순차적으로 연속 설치되는 제1 승온 챔버, 제2 승온 챔버, 제1 열처리 챔버, 제1 냉각 챔버, 제3 승온 챔버, 제2 열처리 챔버와 제2 냉각 챔버를 포함하며, 제1 승온 챔버, 제2 승온 챔버, 제1 열처리 챔버, 제1 냉각 챔버, 제3 승온 챔버, 제2 열처리 챔버와 제2 냉각 챔버 사이에 기밀 밸브, 및 각 챔버 사이에 설치되어 Nd-Fe-B계 소결 자성체를 운반하기 위한 이송 시스템이 설치된다.The continuous heat treatment apparatus includes a first temperature raising chamber, a second temperature raising chamber, a first heat treatment chamber, a first cooling chamber, a third temperature raising chamber, a second heat treatment chamber and a second cooling chamber which are sequentially installed in succession. Nd-Fe-B-based sintering is provided between the chamber, the second temperature raising chamber, the first heat treatment chamber, the first cooling chamber, the third temperature raising chamber, the second heat treatment chamber and the second cooling chamber, and an airtight valve between each chamber. A transport system for transporting the magnetic material is installed.

연속 열처리 과정은 다음과 같다:The continuous heat treatment process is as follows:

(1) 재료 장입(1) charging materials

질량백분율(wt%)에 따라, 조성이 Pr 7.12%, Nd 21.38%, Tb 1.5%, Fe bal., B 0.96%, Cu 0.15%, Ga 0.2%, Nb 0.2%, Co 0.8%인 원료를 취하여, 제련, 스트립 캐스팅, 수소파쇄, 기류파쇄, 압형 및 소결을 통해 Nd-Fe-B계 소결 자성체를 획득한다.According to the mass percentage (wt%), raw materials having a composition of Pr 7.12%, Nd 21.38%, Tb 1.5%, Fe bal., B 0.96%, Cu 0.15%, Ga 0.2%, Nb 0.2%, Co 0.8% Nd-Fe-B-based sintered magnetic bodies are obtained through smelting, strip casting, hydrogen crushing, air crushing, pressing and sintering.

검출을 거친 Nd-Fe-B계 소결 자성체의 성능은 Hcj=16.50kOe, Br=14.2kGs이고, 직각도는 97%이다.The performance of the detected Nd-Fe-B-based sintered magnetic body was Hcj = 16.50 kOe, Br = 14.2 kGs, and the squareness was 97%.

Nd-Fe-B계 소결 자성체를 그리드 재료 박스 내에 담고, 재료 박스를 1열로 적층한 후, 재료 홀더에 배치하여 제1 승온 챔버 내로 이송한다. The Nd-Fe-B-based sintered magnetic body is contained in a grid material box, the material boxes are stacked in one row, and then placed in a material holder and transferred into the first temperature raising chamber.

(2) 제1단계 승온(2) The first stage temperature rise

제1 승온 챔버의 진공도가 150Pa에 도달하였을 때 가열 프로세스를 작동시켜, 실온으로부터 시작하여 150min 동안 승온시키고, 온도가 350℃-380℃에 도달한 후, 30min 동안 보온한다. 보온 종료 후, 재료 박스가 장착된 재료 홀더를 제1 승온 챔버로부터 제2 승온 챔버로 이송한다.The heating process is started when the vacuum degree of the first heating chamber reaches 150 Pa, starting from room temperature for 150 min, warming for 30 min after the temperature reaches 350 ° C.-380 ° C. After the end of heat retention, the material holder with the material box is transferred from the first temperature raising chamber to the second temperature raising chamber.

(3) 제2단계 승온(3) The second stage temperature rise

재료 박스가 장착된 재료 홀더가 제2 승온 챔버로 진입한 후, 진공도가 150Pa에 도달하였을 때, 150min 동안 가열하여 승온시키고, 온도가 820℃-860℃에 도달한 후, 30min 동안 보온한다. 보온 종료 후, 재료 박스가 장착된 재료 홀더를 제2 승온 챔버로부터 제1 열처리 챔버로 이송한다.After the material holder equipped with the material box enters the second temperature raising chamber, when the degree of vacuum reaches 150 Pa, it is heated by heating for 150 minutes, and after the temperature reaches 820 ° C-860 ° C, it is kept warm for 30min. After the end of heat retention, the material holder with the material box is transferred from the second temperature raising chamber to the first heat treatment chamber.

(4) 제1단계 열처리(4) First stage heat treatment

제1 열처리 챔버는 사각형 구조이면서, 사각형 구조 내벽에 서로 반대 방향으로 설치되는 2개의 가열 영역을 포함하며, 가열 영역의 면적은 재료 홀더의 종단면 면적을 초과한다. 재료 박스는 제1 열처리 챔버로 진입한 후, 2개의 가열 영역과 모두 2-30cm의 거리인 위치에 배치되며, 구체적으로는 표 2와 같다.The first heat treatment chamber has a rectangular structure and includes two heating regions installed in opposite directions on the inner wall of the rectangular structure, the area of the heating region exceeding the longitudinal cross-sectional area of the material holder. After entering the first heat treatment chamber, the material box is placed at a position that is a distance of 2-30 cm to both heating regions, specifically, as shown in Table 2.

진공도가 150Pa에 도달하였을 때, 5min 동안 가열하여 승온시키고, 각 영역의 상이한 재료 박스 내의 각기 다른 위치에서 열처리 온도를 검출하여, 구체적으로는 표 2를 참조하며, 175min 동안 보온한다. 보온 종료 후, 재료 박스가 장착된 재료 홀더를 제1단계 열처리 챔버로부터 제1 냉각 챔버로 이송한다.When the degree of vacuum reaches 150 Pa, it is heated for 5 min to raise the temperature, and the heat treatment temperature is detected at different positions in different material boxes in each region, specifically referring to Table 2, and kept warm for 175 min. After the end of the warming, the material holder equipped with the material box is transferred from the first stage heat treatment chamber to the first cooling chamber.

(5) 제1단계 냉각(5) first stage cooling

재료 박스가 장착된 재료 홀더가 제1 냉각 챔버로 진입한 후, 진공시키고, 냉각 챔버로 40-50℃의 76kPa인 불활성 가스를 주입한 다음, 송풍기로 순환 냉각을 실시하며, 냉각 시간은 180min이다. Nd-Fe-B계 소결 자성체의 최초 10min의 평균 냉각 속도는 15℃/min이다. 불활성 가스 온도는 흡기식 순환풍의 공기배출구 부위에서 검출한다.After the material holder equipped with the material box enters the first cooling chamber, it is evacuated, injecting an inert gas of 40-50 ° C. at 76 kPa into the cooling chamber, and then performing circulation cooling with a blower, and the cooling time is 180 min. . The average cooling rate of the first 10 minutes of the Nd-Fe-B-based sintered magnetic body is 15 ° C / min. The inert gas temperature is detected at the air outlet portion of the intake circulation wind.

(6) 제3단계 승온(6) Third stage temperature rise

재료 박스가 장착된 재료 홀더가 제3 승온 챔버로 진입한 후, 진공도가 150Pa에 도달하였을 때, 170min 동안 가열하여 승온시키고, 온도가 380℃-420℃에 이르면 10min 동안 보온한다. 보온 종료 후, 재료 박스가 장착된 재료 홀더를 제3 승온 챔버로부터 제2 열처리 챔버로 이송한다.After the material holder equipped with the material box enters the third temperature raising chamber, when the degree of vacuum reaches 150 Pa, it is heated by heating for 170 min, and is kept warm for 10 min when the temperature reaches 380 ° C-420 ° C. After the end of heat retention, the material holder with the material box is transferred from the third temperature raising chamber to the second heat treatment chamber.

(7) 제2단계 열처리(7) second stage heat treatment

제2 열처리 챔버는 사각형 구조이면서, 사각형 구조 내벽에 서로 반대 방향으로 설치되는 2개의 가열 영역을 포함하며, 가열 영역의 면적은 재료 홀더의 종단면 면적을 초과한다. 재료 박스는 제2 열처리 챔버로 진입한 후, 2개의 가열 영역과 모두 2-30cm의 거리인 위치에 배치되며, 구체적으로는 표 2와 같다.The second heat treatment chamber has a rectangular structure and includes two heating regions installed in opposite directions on the inner wall of the rectangular structure, the area of the heating region exceeding the longitudinal cross-sectional area of the material holder. After entering the second heat treatment chamber, the material box is disposed at a position at a distance of 2-30 cm to both heating regions, specifically, as shown in Table 2 below.

진공도가 150Pa에 도달하였을 때, 10min 동안 가열하여 승온시키고, 각 영역의 상이한 재료 박스 내의 각기 다른 위치에서 열처리 온도를 검출하여, 구체적으로는 표 2를 참조하며, 170min 동안 보온한다. 보온 종료 후, 재료 박스가 장착된 재료 홀더를 제2 열처리 챔버로부터 제2 냉각 챔버로 이송한다.When the degree of vacuum reaches 150 Pa, it is heated for 10 min to raise the temperature, and the heat treatment temperature is detected at different positions in different material boxes in each region, specifically referring to Table 2, and kept for 170 min. After the end of heat retention, the material holder equipped with the material box is transferred from the second heat treatment chamber to the second cooling chamber.

(8) 제2단계 냉각(8) second stage cooling

재료 박스가 장착된 재료 홀더가 제2 냉각 챔버로 진입한 후, 진공시키고, 냉각 챔버로 40-50℃의 76kPa의 불활성 가스를 주입한 다음, 송풍기로 순환 냉각을 실시하며, 냉각 시간은 180min이다. Nd-Fe-B계 소결 자성체의 최초 10min의 평균 냉각 속도는 9.0℃/min이며, 재료 박스가 장착된 재료 홀더를 로에서 인출한다. 불활성 가스 온도는 흡기식 순환풍의 공기배출구 부위에서 검출한다.After the material holder equipped with the material box enters the second cooling chamber, it is vacuumed, 76 kPa of inert gas at 40-50 ° C. is injected into the cooling chamber, and then circulated cooling is performed by a blower, and the cooling time is 180 min. . The average cooling rate of the first 10 min of the Nd-Fe-B-based sintered magnetic body is 9.0 ° C / min, and the material holder with the material box is taken out of the furnace. The inert gas temperature is detected at the air outlet portion of the intake circulation wind.

상기 열처리와 냉각 처리를 거친 후의 자석 성능은 표 2를 참조한다. 표 2 중의 거리는 1열로 적층된 재료 박스와 양측 가열 영역 사이의 거리이다.Refer to Table 2 for the magnet performance after the heat treatment and cooling treatment. The distance in Table 2 is the distance between the material boxes laminated in one row and the heating regions on both sides.

상이한 영역으로부터 20개의 Nd-Fe-B계 소결 자성체를 취하여, 이들의 Br, Hcj, BH(max)와 SQ를 측정하고, 일치성츨 측정하였다. 일치성은 제품 성능 지표의 파동성으로 묘사하며, 파동성은 (최대값-최소값)/최소값으로 정의한다. 파동성이 작을수록 일치성이 양호하다.Twenty Nd-Fe-B-based sintered magnetic bodies were taken from different regions, and these Br, Hcj, BH (max) and SQ were measured, and the conformity was measured. Consistency is described as the wave performance of the product performance indicator, and wave property is defined as (maximum value-minimum value) / minimum value. The smaller the wave, the better the match.

표 2: 제1단계, 제2단계 열처리의 열처리 온도, 및 열처리와 냉각처리 후의 자석 성능Table 2: Heat treatment temperatures of the first and second heat treatments and magnet performance after heat treatment and cooling treatment
항목
Item 제1단계 열처리First stage heat treatment 제2단계 열처리Second stage heat treatment 열처리와 냉각처리 후After heat treatment and cooling treatment 거리(cm)Distance (cm) 열처리온도(℃)Heat treatment temperature (℃) 거리(cm)Distance (cm) 열처리온도(℃)Heat treatment temperature (℃) Br 파동성(%)Br wave (%) Hcj 파동성(%)Hcj Viability (%) SQ 파동성(%)SQ Waveability (%) 실시예2.1Example 2.1 3030 865-880865-880 3030 500-525500-525 0.600.60 55 44 실시예2.2Example 2.2 2525 870-885870-885 2525 515-535515-535 0.580.58 33 33 실시예2.3Example 2.3 2020 880-890880-890 2020 530-540530-540 0.610.61 2.012.01 2.52.5 실시예2.4Example 2.4 1010 890-895890-895 1010 540-545540-545 0.580.58 1.051.05 22 실시예2.5Example 2.5 55 895-900895-900 55 545-550545-550 0.600.60 1.051.05 22 실시예2.6Example 2.6 22 895-910895-910 22 545-560545-560 0.560.56 66 77 실시예2.7Example 2.7 3030 865-880865-880 1010 540-545540-545 0.600.60 1.151.15 22

표2에서 볼 수 있듯이, 제2단계 열처리 온도의 파동이 작을수록, Br은 기본적으로 안정을 유지하고, Hcj와 SQ의 파동성이 모두 작아졌다. 그 이유는 제2단계 열처리 온도가 자성체의 입계 미세조직 위상성분 및 분포와 밀접한 관련이 있기 때문이며, 온도 파동이 클수록 성능 파동이 커진다.As can be seen from Table 2, as the wave of the second stage heat treatment temperature is smaller, Br is basically stable, and both of the waves Hcj and SQ are smaller. The reason is that the second stage heat treatment temperature is closely related to the grain boundary microstructure phase component and distribution of the magnetic material. The larger the temperature fluctuation, the larger the performance wave.

미세조직의 상태는 NdFeB의 성능에 매우 큰 영향을 미치며, 미세조직이 균일할수록, 또한 결정립이 미세할수록 소재의 성능이 우수해지고 성능의 일치성이 높아진다. 소결 NdFeB 재료의 미세조직의 최적화는 주로 열처리 단계에서 발생하며, 따라서 열처리 공정이 재료의 성능에 미치는 영향이 매우 크다. 동일한 조성이라도 열처리 공정이 다르면 자기 성능이 천차만별일 수 있기 때문에, 본 발명은 온도의 균일성 증가를 토대로 조직의 균일성을 높인 다음, 신속한 냉각 속도를 통해 조직을 균일하게 경화시켜, 매 제품의 조직을 균일하게 일치시킴으로써, 재료의 성능과 균일성을 향상시키는 목적을 달성한다.The state of the microstructure has a great influence on the performance of NdFeB. The more uniform the microstructure and the finer the grain, the better the performance of the material and the higher the performance match. Optimization of the microstructure of the sintered NdFeB material occurs mainly in the heat treatment step, and therefore the heat treatment process has a great influence on the performance of the material. Since even if the heat treatment process is different in the same composition, the magnetic performance can vary widely. Therefore, the present invention improves the uniformity of the tissue based on the increase in temperature uniformity, and then uniformly hardens the tissue through a rapid cooling rate, thereby ensuring the structure of every product. By uniformly matching the above, the object of improving the performance and uniformity of the material is achieved.

실시예Example 3 3

연속 열처리 장치는 순차적으로 연속 설치되는 제1 승온 챔버, 제2 승온 챔버, 제1 열처리 챔버, 제1 냉각 챔버, 제3 승온 챔버, 제2 열처리 챔버와 제2 냉각 챔버를 포함하며, 제1 승온 챔버, 제2 승온 챔버, 제1 열처리 챔버, 제1 냉각 챔버, 제3 승온 챔버, 제2 열처리 챔버와 제2 냉각 챔버 사이에 기밀 밸브, 및 각 챔버 사이에 설치되어 Nd-Fe-B계 소결 자성체를 운반하기 위한 이송 시스템이 설치된다.The continuous heat treatment apparatus includes a first temperature raising chamber, a second temperature raising chamber, a first heat treatment chamber, a first cooling chamber, a third temperature raising chamber, a second heat treatment chamber, and a second cooling chamber which are sequentially installed in succession. Chamber, second heating chamber, first heat treatment chamber, first cooling chamber, third heating chamber, a gas tight valve between the second heat treatment chamber and the second cooling chamber, and is installed between each chamber and sintered Nd-Fe-B-based A transport system for transporting the magnetic material is installed.

연속 열처리 과정은 다음과 같다:The continuous heat treatment process is as follows:

(1) 재료 장입(1) charging materials

질량백분율(wt%)에 따라, 조성이 Pr 8%, Nd 19%-21.5%(표 3 중의 TRE에 따라 조정), Tb 1.5%, Fe bal., B 0.97%, Cu 0.1%, Ga 0.1%, Nb 0.1%, Co 1%인 원료를 취하여, 제련, 스트립 캐스팅, 수소파쇄, 기류파쇄, 압형 및 소결을 통해 Nd-Fe-B계 소결 자성체를 획득한다. TRE 함량의 함량비율과 자석 성능은 표 3과 같다.According to the mass percentage (wt%), the composition is Pr 8%, Nd 19% -21.5% (adjusted according to TRE in Table 3), Tb 1.5%, Fe bal., B 0.97%, Cu 0.1%, Ga 0.1% Taking a raw material of 0.1% Nb and 1% Co, Nd-Fe-B-based sintered magnetic body is obtained through smelting, strip casting, hydrogen crushing, air flow crushing, pressing and sintering. The content ratio of the TRE content and the magnet performance are shown in Table 3.

Nd-Fe-B계 소결 자성체를 그리드 재료 박스 내에 담고, 재료 박스를 1열로 적층한 후, 재료 홀더에 배치하여 제1 승온 챔버 내로 이송한다. The Nd-Fe-B-based sintered magnetic body is contained in a grid material box, the material boxes are stacked in one row, and then placed in a material holder and transferred into the first temperature raising chamber.

(2) 제1단계 승온(2) The first stage temperature rise

제1 승온 챔버의 진공도가 10-1Pa에 도달하였을 때 가열 프로세스를 작동시켜, 실온으로부터 시작하여 130min 동안 승온시키고, 온도가 360℃-400℃에 도달한 후, 20min 동안 보온한다. 보온 종료 후, 재료 박스가 장착된 재료 홀더를 제1 승온 챔버로부터 제2 승온 챔버로 이송한다.The heating process is activated when the vacuum degree of the first heating chamber reaches 10 −1 Pa, starting at room temperature for 130 min, warming for 20 min after the temperature reaches 360 ° C.-400 ° C. After the end of heat retention, the material holder with the material box is transferred from the first temperature raising chamber to the second temperature raising chamber.

(3) 제2단계 승온(3) The second stage temperature rise

재료 박스가 장착된 재료 홀더가 제2 승온 챔버로 진입한 후, 진공도가 10-1Pa에 도달하였을 때, 130min 동안 가열하여 승온시키고, 온도가 810℃-830℃에 도달한 후, 20min 동안 보온한다. 보온 종료 후, 재료 박스가 장착된 재료 홀더를 제2 승온 챔버로부터 제1 열처리 챔버로 이송한다.After the material holder equipped with the material box enters the second temperature raising chamber, when the degree of vacuum reaches 10 −1 Pa, it is heated by heating for 130 min, and after the temperature reaches 810 ° C.-830 ° C., it is kept warm for 20 min. do. After the end of heat retention, the material holder with the material box is transferred from the second temperature raising chamber to the first heat treatment chamber.

(4) 제1단계 열처리(4) First stage heat treatment

제1 열처리 챔버는 사각형 구조이면서, 사각형 구조의 내벽에 서로 반대 방향으로 설치되는 2개의 가열 영역을 포함하며, 가열 영역의 면적은 재료 홀더의 종단면 면적을 초과한다. 재료 박스가 장착된 재료 홀더는 제1 열처리 챔버로 진입한 후, 2개의 가열 영역과 모두 5cm의 거리인 위치에 배치된다.The first heat treatment chamber has a rectangular structure and includes two heating regions installed in opposite directions on the inner wall of the rectangular structure, the area of the heating region exceeding the longitudinal cross-sectional area of the material holder. The material holder on which the material box is mounted is placed in a position at a distance of 5 cm from both heating zones after entering the first heat treatment chamber.

진공도가 10-1Pa에 도달하였을 때, 10min 동안 가열하여 승온시키고, 제1 열처리 챔버의 열처리 온도(상이한 재료 박스 내의 각기 다른 위치에서 검출한다)가 905℃-910℃에 이른 후, 140min 동안 보온한다. 보온 종료 후, 재료 박스가 장착된 재료 홀더를 제1단계 열처리 챔버로부터 제1 냉각 챔버로 이송한다.When the degree of vacuum reaches 10 -1 Pa, it is heated for 10 min to raise the temperature, and after the heat treatment temperature (detected at different positions in different material boxes) of the first heat treatment chamber reaches 905 ° C-910 ° C, it is kept warm for 140min. do. After the end of the warming, the material holder equipped with the material box is transferred from the first stage heat treatment chamber to the first cooling chamber.

(5) 제1단계 냉각(5) first stage cooling

재료 박스가 장착된 재료 홀더가 제1 냉각 챔버로 진입한 후, 진공도가 10-1Pa에 도달하였을 때, 냉각 챔버로 70-90℃의 80kPa인 불활성 가스를 주입한 다음, 송풍기로 순환 냉각을 실시하며, 냉각 시간은 150min이다. Nd-Fe-B계 소결 자성체의 최초 10min의 평균 냉각 속도는 6.5℃/min이다. 불활성 가스 온도는 흡기식 순환풍의 공기배출구 부위에서 검출한다.After the material holder equipped with the material box enters the first cooling chamber, when the vacuum degree reaches 10 -1 Pa, inert gas of 70-90 ° C. and 80 kPa is injected into the cooling chamber, and then circulating cooling is performed by the blower. The cooling time is 150 min. The average cooling rate of the first 10 min of the Nd-Fe-B-based sintered magnetic body is 6.5 ° C / min. The inert gas temperature is detected at the air outlet portion of the intake circulation wind.

(6) 제3단계 승온(6) Third stage temperature rise

재료 박스가 장착된 재료 홀더가 제3 승온 챔버로 진입한 후, 진공도가 10-1Pa에 도달하였을 때, 140min 동안 가열하여 승온시키고, 온도가 400℃-425℃에 이르면 10min 동안 보온한다. 보온 종료 후, 재료 박스가 장착된 재료 홀더를 제3 승온 챔버로부터 제2 열처리 챔버로 이송한다.After the material holder equipped with the material box enters the third temperature raising chamber, when the degree of vacuum reaches 10 −1 Pa, it is heated for 140 min to raise the temperature, and when the temperature reaches 400 ° C.-425 ° C., it is kept warm for 10 min. After the end of heat retention, the material holder with the material box is transferred from the third temperature raising chamber to the second heat treatment chamber.

(7) 제2단계 열처리(7) second stage heat treatment

제2 열처리 챔버는 사각형 구조이면서, 사각형 구조의 내벽에 서로 반대 방향으로 설치되는 2개의 가열 영역을 포함하며, 가열 영역의 면적은 재료 홀더의 종단면 면적을 초과한다. 재료 박스가 장착된 재료 홀더는 제2 열처리 챔버로 진입한 후, 2개의 가열 영역과 모두 5cm의 거리인 위치에 배치된다.The second heat treatment chamber has a rectangular structure and includes two heating regions installed in opposite directions on the inner wall of the rectangular structure, the area of the heating region exceeding the longitudinal cross-sectional area of the material holder. The material holder on which the material box is mounted is placed in a position at a distance of 5 cm from both heating zones after entering the second heat treatment chamber.

재료 박스가 장착된 재료 홀더가 제2 열처리 챔버로 진입한 후, 진공도가 10-1Pa에 도달하였을 때, 10min 동안 가열하여 승온시키고, 제2 열처리 챔버의 열처리 온도(상이한 재료 박스 내의 각기 다른 위치에서 검출한다)가 535℃-540℃에 이른 후, 140min 동안 보온한다. 보온 종료 후, 재료 박스가 장착된 재료 홀더를 제2 열처리 챔버로부터 제2 냉각 챔버로 이송한다.After the material holder equipped with the material box enters the second heat treatment chamber, when the vacuum degree reaches 10 −1 Pa, it is heated for 10 min to raise the temperature, and the heat treatment temperature of the second heat treatment chamber (different positions in different material boxes) At 535 ° C.-540 ° C., and keep warm for 140 min. After the end of heat retention, the material holder equipped with the material box is transferred from the second heat treatment chamber to the second cooling chamber.

(8) 제2단계 냉각(8) second stage cooling

재료 박스가 장착된 재료 홀더가 제2 냉각 챔버로 진입한 후, 진공도가 10-1Pa에 도달하였을 때, 냉각 챔버로 30-60℃의 80kPa인 불활성 가스를 주입한 다음, 송풍기로 순환 냉각을 실시하며, 냉각 시간은 150min이다. Nd-Fe-B계 소결 자성체의 최초 10min의 평균 냉각 속도는 6.0℃/min이며, 재료 박스가 장착된 재료 홀더를 로에서 인출한다. 불활성 가스 온도는 흡기식 순환풍의 공기배출구 부위에서 검출한다.After the material holder equipped with the material box enters the second cooling chamber, when the vacuum degree reaches 10 -1 Pa, an inert gas of 80-kPa at 30-60 ° C is injected into the cooling chamber, and then circulating cooling is performed by a blower. The cooling time is 150 min. The average cooling rate of the first 10 min of the Nd-Fe-B-based sintered magnetic body is 6.0 deg. C / min, and the material holder with the material box is taken out of the furnace. The inert gas temperature is detected at the air outlet portion of the intake circulation wind.

상기 열처리와 냉각 처리를 거친 후의 자석 성능은 표 3과 같다.The magnet performance after the heat treatment and cooling treatment is shown in Table 3.

표 3: TRE 함량, 및 열처리와 냉각 처리 전후의 자석 성능Table 3: TRE content and magnet performance before and after heat treatment and cooling
항목
Item TRE 함량(wt%)TRE content (wt%) 열처리 및 냉각처리 전Before heat treatment and cooling 열처리 및 냉각처리 후After heat treatment and cooling treatment Br
(kGs)Br
(kGs) Hcj
(KOe)Hcj
(KOe) SQ
(%)SQ
(%) Br 파동성(%)Br wave (%) Hcj
파동성(%)Hcj
Oscillation (%) SQ 파동성(%)SQ Waveability (%) 실시예3.1Example 3.1 31.031.0 14.0014.00 22.0122.01 9898 0.650.65 1.381.38 33 실시예3.2Example 3.2 30.530.5 14.1014.10 21.821.8 9999 0.580.58 1.581.58 22 실시예3.3Example 3.3 29.529.5 14.2514.25 21.221.2 9999 0.600.60 1.631.63 22 실시예3.4Example 3.4 28.828.8 14.3014.30 2121 9898 0.630.63 1.851.85 22 비교예3.1Comparative Example 3.1 28.528.5 14.3614.36 20.120.1 9696 0.720.72 1.981.98 55

열처리 및 냉각 처리 전의 자석의 Br 파동성(%), Hcj 파동성(%)과 SQ 파동성(%)은 0이다.The Br wave (%), Hcj wave (%) and SQ wave (%) of the magnets before heat treatment and cooling were zero.

종래의 열처리 과정에서, 일반적으로, TRE가 30.5%를 초과하는 자석은 열처리 과정에서 일치성이 비교적 양호한 반면, TRE가 28.8wt%-30.5%인 자석은 열처리 과정에서, Br 파동성(%), Hcj 파동성(%)과 SQ 파동성(%) 중의 하나 이상의 항목이 5% 이상에 달할 수 있어 제품의 일치성에 영향을 미친다.In the conventional heat treatment process, in general, magnets having a TRE of more than 30.5% have a relatively good agreement in the heat treatment process, whereas magnets having a TRE of 28.8 wt% -30.5% have a Br wave (%), At least one item of Hcj wave% and SQ wave% can reach 5% or more, affecting product consistency.

본 출원인은 TRE가 28.8wt%-30.5%인 자석을 상기 온도차가 비교적 작고, 최초 10min의 평균 냉각 속도가 제어되는 열처리 장치에서 열처리를 하는 경우, Br 파동성(%), Hcj 파동성(%)과 SQ 파동성(%)이 모두 감소하여 일치성이 현저하게 향상될 수 있음을 발견하였다.The Applicant said that when the magnet having a TRE of 28.8wt% -30.5% is heat-treated in a heat treatment apparatus in which the temperature difference is relatively small and the average cooling rate of the first 10min is controlled, Br wave property (%) and Hcj wave property (%) It was found that both the and SQ wave characteristics (%) could be reduced to significantly improve the consistency.

도 3에서 볼 수 있듯이, 평면 열처리 장치의 온도 균일성을 높이고, 그 냉각 속도를 제어할 경우, 희토류 함량이 낮은 네오디움의 성능을 향상시키는데 매우 중요한 긍정적 효과를 갖는다. As can be seen in Figure 3, when increasing the temperature uniformity of the planar heat treatment apparatus, and controlling the cooling rate, it has a very important positive effect to improve the performance of neodymium with a low rare earth content.

비교예Comparative example

연속 열처리 장치는 순차적으로 연속 설치되는 제1 열처리 챔버와 제2 열처리 챔버를 포함하며, 제1 열처리 챔버와 제2 열처리 챔버 사이에 기밀 밸브, 및 Nd-Fe-B계 소결 자성체를 운반하기 위해 두 챔버 사이에 설치되는 이송 시스템이 설치된다.The continuous heat treatment apparatus includes a first heat treatment chamber and a second heat treatment chamber that are sequentially installed in succession, wherein the airtight valve and the Nd-Fe-B-based sintered magnetic body are carried between the first heat treatment chamber and the second heat treatment chamber. A transfer system is installed between the chambers.

연속 열처리 과정은 다음과 같다:The continuous heat treatment process is as follows:

질량백분율(wt%)의 조성이 Pr 8%, Nd 20%, Tb 1.5%, Fe bal., B 0.97%, Cu 0.1%, Ga 0.1%, Nb 0.1%, Co 1%인 원료를 취하여, 제련, 스트립 캐스팅, 수소파쇄, 기류파쇄, 압형 및 소결을 통해 Nd-Fe-B계 소결 자성체를 획득하며, 구체적인 공정 파라미터는 실시예3과 동일하다.By smelting the raw material of the mass percentage (wt%) is Pr 8%, Nd 20%, Tb 1.5%, Fe bal., B 0.97%, Cu 0.1%, Ga 0.1%, Nb 0.1%, Co 1% , Nd-Fe-B-based sintered magnetic body was obtained through strip casting, hydrogen crushing, airflow crushing, pressing and sintering, and specific process parameters were the same as in Example 3.

Nd-Fe-B계 소결 자성체를 그리드 재료 박스 내에 담고, 재료 박스를 1열로 적층한 후, 재료 홀더에 배치하여 제1 열처리 챔버 내로 이송한다.The Nd-Fe-B-based sintered magnetic body is contained in a grid material box, the material boxes are stacked in one row, and then placed in a material holder and transferred into the first heat treatment chamber.

재료 박스가 장착된 재료 홀더는 제1 열처리 챔버로 진입한 후, 2개의 가열영역과 모두 5cm 거리인 위치에 배치되며, 진공도가 10-1Pa에 도달하였을 때, 180min 동안 가열하여 승온시키고, 제1 열처리 챔버의 열처리 온도(상이한 재료 박스 내의 각기 다른 위치에서 검출한다)가 905℃-910℃에 이른 후, 140min 동안 보온한다. 보온 종료 후, 제1 열처리 챔버로 70-90℃의 80kPa의 불활성 가스를 주입한 다음, 송풍기로 순환 냉각을 실시하며, 냉각 시간은 150min이다. 불활성 가스 온도는 흡기식 순환풍의 공기배출구 부위에서 검출한다. Nd-Fe-B계 소결 자성체의 최초 10min의 평균 냉각 속도는 5℃/min이다. 재료 박스 장착된 재료 홀더를 제1 열처리 챔버로부터 제2 열처리 챔버로 이송한다.After entering the first heat treatment chamber, the material holder equipped with the material box is placed at a position 5 cm away from the two heating zones. When the vacuum degree reaches 10 −1 Pa, the material holder is heated and heated for 180 min. 1 After the heat treatment temperature (detected at different positions in different material boxes) of the heat treatment chamber reaches 905 ° C-910 ° C, it is kept warm for 140min. After the end of the warming, 80 kPa of inert gas at 70-90 ° C. was injected into the first heat treatment chamber, followed by circulating cooling with a blower, and the cooling time was 150 min. The inert gas temperature is detected at the air outlet portion of the intake circulation wind. The average cooling rate of the first 10 min of the Nd-Fe-B-based sintered magnetic body is 5 ° C / min. A material box mounted material holder is transferred from the first heat treatment chamber to the second heat treatment chamber.

재료 박스가 장착된 재료 홀더는 제2 열처리 챔버로 진입한 후, 2개의 가열영역과 모두 5cm 거리인 위치에 배치되며, 진공도가 10-1Pa에 도달하였을 때, 90min 동안 가열하여 승온시키고, 제2 열처리 챔버의 열처리 온도(상이한 재료 박스 내의 각기 다른 위치에서 검출한다)가 535℃-540℃에 이른 후, 140min 동안 보온한다. 보온 종료 후, 제2 열처리 챔버로 30-60℃의 80kPa의 불활성 가스를 주입한 다음, 송풍기로 순환 냉각을 실시하며, 냉각 시간은 150min이다. 불활성 가스 온도는 흡기식 순환풍의 공기배출구 부위에서 검출한다. Nd-Fe-B계 소결 자성체의 최초 10min의 평균 냉각 속도는 4.5℃/min이다. After entering the second heat treatment chamber, the material holder equipped with the material box is placed at a position 5 cm away from the two heating zones. When the vacuum degree reaches 10 −1 Pa, the material holder is heated and heated for 90 min. 2 After the heat treatment temperature (detected at different positions in different material boxes) of the heat treatment chamber reaches 535 ° C.-540 ° C., it is kept warm for 140 min. After the end of the warming, 80 kPa of inert gas at 30-60 ° C. was injected into the second heat treatment chamber, followed by circulating cooling with a blower, and the cooling time was 150 min. The inert gas temperature is detected at the air outlet portion of the intake circulation wind. The average cooling rate of the first 10 min of the Nd-Fe-B-based sintered magnetic body is 4.5 ° C / min.

표 4: TRE 함량, 및 단일 챔버의 열처리와 냉각처리 전후의 자석 성능Table 4: TRE content and magnet performance before and after heat treatment and cooling in a single chamber
항목
Item TRE 함량
(wt%)TRE content
(wt%) 열처리 및 냉각처리 전Before heat treatment and cooling 열처리 및 냉각처리 후After heat treatment and cooling treatment Br(kGs)Br (kGs) Hcj(KOe)Hcj (KOe) SQ(%)SQ (%) Br 파동성(%)Br wave (%) Hcj 파동성(%)Hcj Viability (%) SQ 파동성(%)SQ Waveability (%) 비교예4.1Comparative Example 4.1 29.529.5 14.2514.25 21.221.2 9999 0.660.66 88 55

열처리 및 냉각처리 전의 자석의 Br 파동성(%), Hcj 파동성(%)과 SQ 파동성(%)을 0으로 설정한다.Br wave characteristics (%), Hcj wave characteristics (%) and SQ wave characteristics (%) of the magnets before heat treatment and cooling treatment are set to zero.

표 3과 표 4에서 볼 수 있듯이, 단일 챔버에서 열처리와 냉각처리를 실시하여, 고온 구간의 냉각 속도가 비교적 낮고, 단일 챔버에서 처리 시의 Br, SQ가 약간 하강하였으며, Hcj의 하강이 비교적 뚜렷하고, 또한 세 가지 항목의 파동성이 뚜렷하게 커졌음을 알 수 있다.As can be seen from Table 3 and Table 4, the heat treatment and cooling treatment were performed in a single chamber, so that the cooling rate of the high temperature section was relatively low, Br and SQ decreased slightly during the treatment in a single chamber, and the drop of Hcj was relatively clear. In addition, it can be seen that the vibration of the three items is significantly increased.

상기 실시예는 단지 본 발명의 몇 가지 구체적인 실시방식을 추가적으로 설명하기 위한 것일 뿐이며, 본 발명은 결코 실시예에 국한되지 않는다. 본 발명의 기술 실질에 의거하여 이상의 실시예에 대해 실시하는 임의의 간단한 수정, 동등한 변화와 수식은 모두 본 발명의 기술방안의 보호 범위 내에 포함된다. The above embodiments are merely intended to further explain some specific embodiments of the present invention, and the present invention is in no way limited to the embodiments. Any simple modifications, equivalent changes, and modifications made to the above embodiments based on the technical substance of the present invention are all included within the protection scope of the technical solution of the present invention.

Claims (12)

합금 공작물 또는 금속 공작물의 연속 열처리 장치에 있어서,
기밀장치를 통해 순차적으로 설치되는 제1 열처리 챔버, 제1 냉각 챔버, 제2 열처리 챔버, 제2 냉각 챔버, 및 상기 합금 공작물 또는 금속 공작물을 이송하기 위해 각 챔버 사이에 설치되는 이송 시스템을 포함하고, 상기 제1 냉각 챔버와 상기 제2 냉각 챔버는 모두 공랭 시스템을 채택하며, 상기 제1 냉각 챔버의 냉각풍 온도는 25℃ 이상이면서, 상기 제1 열처리 챔버의 열처리 온도와 적어도 450℃의 차이가 있고, 상기 제2 냉각 챔버의 냉각풍 온도는 25℃ 이상이면서, 상기 제2 열처리 챔버의 열처리 온도와 적어도 300℃의 차이가 있으며, 상기 냉각 챔버의 압력은 50kPa-100kPa인 것을 특징으로 하는 합금 공작물 또는 금속 공작물의 연속 열처리 장치.In the continuous heat treatment apparatus of an alloy workpiece or a metal workpiece,
A first heat treatment chamber sequentially installed through an airtight device, a first cooling chamber, a second heat treatment chamber, a second cooling chamber, and a transfer system installed between the chambers for transferring the alloy work or the metal work; The first cooling chamber and the second cooling chamber both adopt an air cooling system, and the cooling air temperature of the first cooling chamber is 25 ° C. or more, and the difference between the heat treatment temperature of the first heat treatment chamber and at least 450 ° C. And the cooling air temperature of the second cooling chamber is 25 ° C. or more, and is at least 300 ° C. different from the heat treatment temperature of the second heat treatment chamber, and the pressure of the cooling chamber is 50 kPa-100 kPa. Or continuous heat treatment apparatus for metal workpieces. 제1항에 있어서,
상기 합금 공작물은 Nd-Fe-B계 소결 자성체인 것을 특징으로 하는 합금 공작물 또는 금속 공작물의 연속 열처리 장치.The method of claim 1,
The alloy workpiece is a continuous heat treatment apparatus of an alloy workpiece or a metal workpiece, characterized in that the Nd-Fe-B-based sintered magnetic body. 제1항에 있어서,
상기 공랭 시스템은 불활성 가스를 채택한 공랭 시스템인 것을 특징으로 하는 합금 공작물 또는 금속 공작물의 연속 열처리 장치.The method of claim 1,
And said air-cooling system is an air-cooling system employing an inert gas. 제3항에 있어서,
상기 제1 열처리 챔버의 열처리 온도는 800℃-950℃이고, 상기 제1 냉각 챔버의 냉각풍 온도는 25℃-150℃이며, 상기 제2 열처리 챔버의 열처리 온도는 400℃-650℃이고, 상기 제2 냉각 챔버의 냉각풍 온도는 25℃-100℃인 것을 특징으로 하는 합금 공작물 또는 금속 공작물의 연속 열처리 장치.The method of claim 3,
The heat treatment temperature of the first heat treatment chamber is 800 ℃-950 ℃, the cooling wind temperature of the first cooling chamber is 25 ℃-150 ℃, the heat treatment temperature of the second heat treatment chamber is 400 ℃-650 ℃, The cooling wind temperature of the 2nd cooling chamber is 25 degreeC-100 degreeC, The continuous heat processing apparatus of an alloy workpiece or a metal workpiece. 제1항에 있어서,
상기 제1 열처리 챔버는 사각형 구조이면서, 상기 사각형 구조 내벽에 서로 반대 방향으로 설치되는 2개의 가열 영역을 포함하고, 상기 합금 공작물 또는 상기 금속 공작물은 상기 사각형 구조 중앙부의 재료 홀더에 직접 배치되거나, 또는 상기 합금 공작물 또는 상기 금속 공작물은 먼저 재료 박스 내에 담긴 후 상기 재료 박스가 상기 사각형 구조 중앙의 재료 홀더에 배치되며; 마찬가지로, 상기 제2 열처리 챔버는 사각형 구조이면서, 상기 사각형 구조 내벽에 서로 반대 방향으로 설치되는 2개의 가열 영역을 포함하고, 상기 합금 공작물 또는 상기 금속 공작물은 상기 사각형 구조 중앙부의 재료 홀더에 직접 배치되거나, 또는 상기 합금 공작물 또는 상기 금속 공작물은 먼저 재료 박스 내에 담긴 후 상기 재료 박스가 상기 사각형 구조 중앙의 재료 홀더에 배치되는 것을 특징으로 하는 합금 공작물 또는 금속 공작물의 연속 열처리 장치.The method of claim 1,
The first heat treatment chamber has a rectangular structure and includes two heating zones installed in opposite directions on the inner wall of the rectangular structure, and the alloy workpiece or the metal workpiece is disposed directly in a material holder in the center of the rectangular structure, or The alloy workpiece or the metal workpiece is first contained in a material box and then the material box is placed in a material holder in the center of the rectangular structure; Similarly, the second heat treatment chamber has a rectangular structure and includes two heating zones installed in opposite directions on the inner wall of the rectangular structure, and the alloy workpiece or the metal workpiece is disposed directly in a material holder in the center of the rectangular structure. Or the alloy workpiece or the metal workpiece is first contained in a material box and then the material box is placed in a material holder in the center of the rectangular structure. 제5항에 있어서,
상기 가열 영역의 면적은 상기 재료 홀더의 종단면 면적을 초과하는 것을 특징으로 하는 합금 공작물 또는 금속 공작물의 연속 열처리 장치.The method of claim 5,
And the area of the heating zone exceeds the longitudinal cross-sectional area of the material holder. 제1항에 있어서,
상기 제1 열처리 챔버와 제2 열처리 챔버 중, 상기 합금 공작물 또는 상기 금속 공작물 또는 상기 재료 박스로부터 서로 반대 방향으로 설치되는 2개의 상기 가열 영역의 거리는 동일하며, 5cm-20cm인 것을 특징으로 하는 합금 공작물 또는 금속 공작물의 연속 열처리 장치.The method of claim 1,
An alloy workpiece, wherein the distances of the two heating zones provided in opposite directions from the alloy workpiece, the metal workpiece, or the material box among the first heat treatment chamber and the second heat treatment chamber are the same, and are 5 cm-20 cm. Or continuous heat treatment apparatus for metal workpieces. 제7항에 있어서,
상기 Nd-Fe-B계 자성체는 TRE가 28.8wt%-30.5wt%인 Nd-Fe-B계 자성체인 것을 특징으로 하는 합금 공작물 또는 금속 공작물의 연속 열처리 장치.The method of claim 7, wherein
The Nd-Fe-B-based magnetic material is an Nd-Fe-B-based magnetic material having a TRE of 28.8wt% -30.5wt%. 합금 공작물 또는 금속 공작물의 연속 열처리 방법에 있어서,
상호 기밀되는 분리 챔버에서 순차적으로 실시되는 제1단계 열처리, 제1단계 공냉각 처리, 제2단계 열처리, 및 제2단계 공냉각 처리를 포함하며, 상기 제1단계 공냉각 처리의 냉각풍 온도는 25℃ 이상이면서, 상기 제1단계 열처리의 열처리 온도와 적어도 450℃의 차이가 있고, 상기 제2단계 공냉각 처리의 냉각풍 온도는 25℃ 이상이면서, 상기 제2단계 열처리의 열처리 온도와 적어도 300℃의 차이가 있는 것을 특징으로 하는 합금 공작물 또는 금속 공작물의 연속 열처리 방법.In the continuous heat treatment method of an alloy workpiece or a metal workpiece,
A first stage heat treatment, a first stage air cooling treatment, a second stage heat treatment, and a second stage air cooling treatment, which are sequentially performed in the mutually hermetic separation chamber, wherein the cooling wind temperature of the first stage air cooling treatment is 25 ° C. or more, and a difference of at least 450 ° C. from the heat treatment temperature of the first step heat treatment, and a cooling wind temperature of the second step air cooling treatment is 25 ° C. or more, and at least 300 ° C. with the heat treatment temperature of the second step heat treatment. A continuous heat treatment method for an alloy workpiece or a metal workpiece, characterized by a difference in degrees Celsius. 제9항에 있어서,
상기 합금 공작물은 Nd-Fe-B계 소결 자성체인 것을 특징으로 하는 합금 공작물 또는 금속 공작물의 연속 열처리 방법.The method of claim 9,
The alloy workpiece is a continuous heat treatment method of an alloy workpiece or a metal workpiece, characterized in that the Nd-Fe-B-based sintered magnetic material. 제10항에 있어서,
상기 제2단계 열처리 중, 상이한 영역의 상기 합금 공작물 또는 금속 공작물의 온도차는 ±5℃ 이하인 것을 특징으로 하는 합금 공작물 또는 금속 공작물의 연속 열처리 방법.The method of claim 10,
During the second step of heat treatment, the temperature difference between the alloy workpiece or the metal workpiece in different regions is ± 5 ° C. or less. 제9항에 있어서,
상기 제1단계 냉각 처리 중, 상기 합금 공작물 또는 상기 금속 공작물의 최초 10min의 평균 냉각 속도는 6℃/min-15℃/min이고, 상기 합금 공작물 또는 금속 공작물의 상기 제2단계 냉각 처리 중, 최초 10min의 평균 냉각 속도는 6℃/min-15℃/min인 것을 특징으로 하는 합금 공작물 또는 금속 공작물의 연속 열처리 방법.
The method of claim 9,
During the first stage cooling treatment, the average cooling rate of the first 10 min of the alloy workpiece or the metal workpiece is 6 ° C./min-15° C./min, and the first stage of the second stage cooling treatment of the alloy workpiece or the metal workpiece is performed. An average cooling rate of 10 min is 6 ℃ / min-15 ℃ / min method of continuous heat treatment of an alloy workpiece or a metal workpiece.
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